CN106654197A - Preparation method of ternary precursor containing Mg and Al - Google Patents
Preparation method of ternary precursor containing Mg and Al Download PDFInfo
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- CN106654197A CN106654197A CN201611065542.2A CN201611065542A CN106654197A CN 106654197 A CN106654197 A CN 106654197A CN 201611065542 A CN201611065542 A CN 201611065542A CN 106654197 A CN106654197 A CN 106654197A
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- H01M4/00—Electrodes
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/502—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese for non-aqueous cells
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
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Abstract
The invention discloses a preparation method of a ternary precursor containing Mg and Al. The preparation method specifically comprises the following steps: step 1, preparing a ternary solution containing nickel, cobalt and manganese; step 2, adding a complexing agent into the ternary solution of the step 1; step 3, adding a magnesium salt solution and an aluminum salt solution into a mixed solution of the step 2; step 4, adding a sodium hydroxide solution and ammonia water into a mixed solution of the step 3 and finishing precipitation reaction to obtain the ternary precursor containing the Mg and the Al. According to the preparation method disclosed by the invention, magnesium and aluminum doping elements are directly added into the nickel-cobalt-manganese ternary solution and the doping elements are stabilized by adding the complexing agent; precipitation speed difference of all metal ions in a reaction system is reduced, and uniform co-precipitation is realized; the doping elements can be uniformly distributed into precursor particles, so that the effect of a doping element stabilizing structure is sufficiently expressed; the problem that the discharge capacity is reduced, caused by doping, is reduced to the minimum, and the balance of the discharge specific capacity and the structure stability is realized.
Description
Technical field
The invention belongs to ternary precursor fabricating technology field, and in particular to a kind of ternary forerunner containing Mg, Al
The preparation method of body.
Background technology
Nickel-cobalt-manganese ternary anode material for lithium-ion batteries is due to higher energy density and relatively low price
It is widely used in IT product and new-energy automobile field.But simple nickle cobalt lithium manganate (LNCM) is owed due to structural stability
It is good, it is easy in charge and discharge process because the deintercalation of Li ions and the change of Ni, Co, Mn ionic valence condition cause material structure
Subside, the cycle life and safety to material causes greatly harm.For these problems typically using mix appropriate Mg,
The mode of Al ions improves, traditional Mg, Al doping way be after presoma operation, by solid phase mixing mix MgO and
Al2O3, this method is although simple to operation, but can produce the uneven problem of mixing unavoidably, causes local Mg, Al content inclined
Height, specific discharge capacity significantly deteriorates and other positions meeting contents are low, and cycle life cannot be effectively improved.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the ternary precursor containing Mg, Al, is preparing ternary forerunner
Doped chemical is added during body, and doped chemical is formed with host element by adding chelating agent and the suitable process conditions of control
Uniform co-precipitation, realizes that atom level mixes.
The technical solution adopted in the present invention is that a kind of preparation method of the ternary precursor containing Mg, Al is specifically included
Following steps：
Step 1, configure containing nickel, cobalt, manganese ternary solution；
Step 2, to adding chelating agent in the ternary solution described in step 1；
Step 3, to addition magnesium salt solution and aluminum salt solution in the mixed solution described in step 2；
Step 4, will add sodium hydroxide solution and ammonia in the mixed solution described in step 3, complete precipitation, i.e.,
Obtain the ternary precursor containing Mg, Al.
Of the invention the characteristics of, also resides in,
Step 2 complexing agent be 1,10- orthophenanthrolines, disodiumedetate, dimercaptopropanol, BAL, dimercaptopropane sulphur
Sour sodium, mercaptoethylmaine, TGA, thiourea, ammonium fluoride, 8-hydroxyquinoline, potassium cyanide, acetylacetone,2,4-pentanedione, citric acid, tartaric acid,
Oxalic acid, sulfosalicylic acid, triethanolamine, double (the 2- amino-ethyl ethers) tetraacethyls of ethylene glycol, ethylenediamine tetrapropionic acid, triethylenetetramine
In one or more combination.
The addition of step 2 complexing agent is the 0.1%-10% of nickel, cobalt and manganese gross mass.
Magnesium salt is one or more the combination in magnesium chloride, magnesium acetate, magnesium sulfate, magnesium nitrate in step 3.
Aluminium salt is the one kind in aluminum chloride, aluminium acetate, aluminum isopropylate., normal propyl alcohol aluminum, aluminum sulfate, aluminum nitrate in step 3
Or more than one combination.
The incorporation of magnesium salt is the 0.001%-2% of nickel, cobalt and manganese gross mass in step 3, and the incorporation of aluminium salt is nickel, cobalt
With the 0.001%-2% of manganese gross mass.
The flow-rate ratio of mixed solution, sodium hydroxide solution and ammonia is 1.8～2.2 in step 4：1.8～2.2：1.
The molar concentration of sodium hydroxide solution is 4mol/L, and the molar concentration of ammonia is 6mol/L.
Precipitation in step 4 is carried out in a kettle., and reaction temperature is：70～80 DEG C, the response time is：22～36h.
The invention has the beneficial effects as follows, a kind of preparation method of the ternary precursor containing Mg, Al of the present invention, by nickel
Magnesium, aluminum doped chemical are directly added in cobalt-manganese ternary solution, and by adding the stable doped chemical of chelating agent, and reduce each metal
Settling velocity difference of the ion in reaction system, realizes uniform co-precipitation, enables doped chemical to be evenly distributed in forerunner
In body granule, so as to give full play to the effect of doped chemical rock-steady structure, and the discharge capacity that doping is brought reduces problem and subtracts
Little is minimum, realizes the balance of specific discharge capacity and structural stability.
Description of the drawings
Fig. 1 provides the capacity pair of the ternary precursor that conventional method is prepared with the inventive method in embodiment 1 for the present invention
Than figure；
Fig. 2 provides the capacity pair of the ternary precursor that conventional method is prepared with the inventive method in embodiment 2 for the present invention
Than figure；
Fig. 3 provides the capacity pair of the ternary precursor that conventional method is prepared with the inventive method in embodiment 3 for the present invention
Than figure.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that specific embodiment described herein is not used to only to explain the present invention
Limit the present invention.
The embodiment of the present invention provides a kind of preparation method of the ternary precursor containing Mg, Al, specifically includes following steps：
Step 1, configure containing nickel, cobalt, manganese ternary solution；
Nickel, cobalt, the mol ratio of manganese are：1：0.3～0.5：0.5～0.7；
Step 2, to adding chelating agent in the ternary solution described in step 1；
Chelating agent is 1,10- orthophenanthrolines, disodiumedetate, dimercaptopropanol, BAL, Sodium Dimercapto Sulfonate, mercapto
Base ethamine, TGA, thiourea, ammonium fluoride, 8-hydroxyquinoline, potassium cyanide, acetylacetone,2,4-pentanedione, citric acid, tartaric acid, oxalic acid, sulphur
Base salicylic acid, triethanolamine, double (the 2- amino-ethyl ethers) tetraacethyls of ethylene glycol, ethylenediamine tetrapropionic acid, in triethylenetetramine
Plant or more than one combination；
The addition of chelating agent is the 0.1%-10% of nickel, cobalt and manganese gross mass；
Step 3, to addition magnesium salt solution and aluminum salt solution in the mixed solution described in step 2；
Magnesium salt is one or more the combination in magnesium chloride, magnesium acetate, magnesium sulfate, magnesium nitrate；Aluminium salt is trichlorine
Change one or more the combination in aluminum, aluminium acetate, aluminum isopropylate., normal propyl alcohol aluminum, aluminum sulfate, aluminum nitrate；Magnesium salt is mixed
Enter the 0.001%-2% that amount is nickel, cobalt and manganese gross mass, the incorporation of aluminium salt is the 0.001%- of nickel, cobalt and manganese gross mass
2%；
Step 4, will add sodium hydroxide solution and ammonia in the mixed solution described in step 3, complete precipitation, i.e.,
Obtain the ternary precursor containing Mg, Al；
Wherein, the flow-rate ratio of mixed solution, sodium hydroxide solution and ammonia is 1.8～2.2：1.8～2.2：1；It is described
The molar concentration of sodium hydroxide solution is 4mol/L, and the molar concentration of ammonia is 6mol/L；Precipitation is carried out in a kettle.,
Reaction temperature is：70～80 DEG C, the response time is：22～36h.
Compare compared with preparation method, the present invention mainly has following technical advantage：By straight in nickel-cobalt-manganese ternary solution
Connect addition magnesium, aluminum doped chemical, and by adding the stable doped chemical of chelating agent, and reduce each metal ion in reaction system
Settling velocity difference, realize uniform co-precipitation, doped chemical is evenly distributed in granular precursor, so as to abundant
The effect of doped chemical rock-steady structure is played, and the discharge capacity that doping is brought reduces minimum, the realization electric discharge that problem reduces
The balance of specific capacity and structural stability.
Embodiment 1
Nickel cobalt manganese mol ratio to 2mol/L is 55:25:Double (the 2- amino of ethylene glycol of 5g/L are added in 20 ternary solution
Ethylether) tetraacethyl, the magnesium sulfate of 0.5g/L and the aluminum chloride of 0.5g/L are then respectively adding, it is sufficiently stirred for dissolving；With
The sodium hydroxide solution of 4mol/L and the ammonia spirit of 6mol/L are according to 1.8:1.8:1 flow-rate ratio is added by dosing pump cocurrent
Enter in reactor, 70 DEG C of reaction temperature, the response time is 22h, obtain a kind of ternary precursor containing Mg, Al.
By above-mentioned ternary precursor and identical synthesis condition, identical magnalium doping, the ternary being prepared by a conventional method
Presoma is circulated life span comparison's test, and test result is shown in Fig. 1.From figure 1 it appears that the inventive method (Liquid
Fase doping) prepare ternary precursor, under the identical life-span, its capacity be more than conventional method (Solid fase
Doping) the ternary precursor for preparing.
Embodiment 2
Nickel cobalt manganese mol ratio to 2mol/L is 5:2:The oxalic acid of 5g/L is added in 3 ternary solution, is then respectively adding
The magnesium nitrate of 0.3g/L and the aluminum sulfate of 1.0g/L, are sufficiently stirred for dissolving；With the sodium hydroxide solution and 6mol/L of 4mol/L
Ammonia spirit according to 2:2:1 flow-rate ratio is added in reactor by dosing pump cocurrent, 75 DEG C of reaction temperature, the response time
For 24h, a kind of ternary precursor containing Mg, Al is obtained.
By above-mentioned ternary precursor and identical synthesis condition, identical magnalium doping, the ternary being prepared by a conventional method
Presoma is circulated life span comparison's test, and test result is shown in Fig. 2.From figure 2 it can be seen that ternary forerunner prepared by the present invention
Body, under the identical life-span, its capacity is more than ternary precursor prepared by conventional method.
Embodiment 3
Nickel cobalt manganese mol ratio to 2mol/L is 6:2:The Sodium Dimercapto Sulfonate of 10g/L is added in 2 ternary solution,
The magnesium chloride of 1.0g/L and the aluminum chloride of 1.5g/L are then respectively adding, dissolving is sufficiently stirred for；With the sodium hydroxide of 4mol/L
The ammonia spirit of solution and 6mol/L is according to 1.9:2:1 flow-rate ratio is added in reactor by dosing pump cocurrent, reaction
Temperature 70 C, the response time is 36h, obtains a kind of ternary precursor containing Mg, Al.
By above-mentioned ternary precursor and identical synthesis condition, identical magnalium doping, the ternary being prepared by a conventional method
Presoma is circulated life span comparison's test, and test result is shown in Fig. 3.From figure 3, it can be seen that ternary forerunner prepared by the present invention
Body, under the identical life-span, its capacity is more than ternary precursor prepared by conventional method.
The above, only presently preferred embodiments of the present invention is not intended to limit protection scope of the present invention.
Claims (10)
1. a kind of preparation method of the ternary precursor containing Mg, Al, it is characterised in that specifically include following steps：
Step 1, configure containing nickel, cobalt, manganese ternary solution；
Step 2, to adding chelating agent in the ternary solution described in step 1；
Step 3, to addition magnesium salt solution and aluminum salt solution in the mixed solution described in step 2；
Step 4, will add sodium hydroxide solution and ammonia in the mixed solution described in step 3, complete precipitation, that is, obtain
Ternary precursor containing Mg, Al.
2. the preparation method of a kind of ternary precursor containing Mg, Al according to claim 1, it is characterised in that described
Nickel, cobalt, the mol ratio of manganese are in step 1：1：0.3～0.5：0.5～0.7.
3. the preparation method of a kind of ternary precursor containing Mg, Al according to claim 1, it is characterised in that described
Step 2 complexing agent be 1,10- orthophenanthrolines, disodiumedetate, dimercaptopropanol, BAL, Sodium Dimercapto Sulfonate, mercapto
Base ethamine, TGA, thiourea, ammonium fluoride, 8-hydroxyquinoline, potassium cyanide, acetylacetone,2,4-pentanedione, citric acid, tartaric acid, oxalic acid, sulphur
Base salicylic acid, triethanolamine, double (the 2- amino-ethyl ethers) tetraacethyls of ethylene glycol, ethylenediamine tetrapropionic acid, in triethylenetetramine
Plant or more than one combination.
4. the preparation method of a kind of ternary precursor containing Mg, Al according to claim 3, it is characterised in that described
The addition of step 2 complexing agent is the 0.1%-10% of nickel, cobalt and manganese gross mass.
5. the preparation method of a kind of ternary precursor containing Mg, Al according to claim 1, it is characterised in that described
Magnesium salt is one or more the combination in magnesium chloride, magnesium acetate, magnesium sulfate, magnesium nitrate in step 3.
6. the preparation method of a kind of ternary precursor containing Mg, Al according to claim 1, it is characterised in that described
In step 3 aluminium salt be aluminum chloride, aluminium acetate, aluminum isopropylate., normal propyl alcohol aluminum, aluminum sulfate, aluminum nitrate in one kind or one kind with
On combination.
7. the preparation method of a kind of ternary precursor containing Mg, Al according to claim 1, it is characterised in that described
The incorporation of magnesium salt is the 0.001%-2% of nickel, cobalt and manganese gross mass in step 3, and the incorporation of aluminium salt is the total matter of nickel, cobalt and manganese
The 0.001%-2% of amount.
8. the preparation method of a kind of ternary precursor containing Mg, Al according to claim 1, it is characterised in that described
The flow-rate ratio of mixed solution, sodium hydroxide solution and ammonia is 1.8～2.2 in step 4：1.8～2.2：1.
9. the preparation method of a kind of ternary precursor containing Mg, Al according to claim 8, it is characterised in that described
The molar concentration of sodium hydroxide solution is 4mol/L, and the molar concentration of ammonia is 6mol/L.
10. the preparation method of a kind of ternary precursor containing Mg, Al according to claim 9, it is characterised in that described
Precipitation in step 4 is carried out in a kettle., and reaction temperature is：70～80 DEG C, the response time is 22～36h.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107500366A (en) * | 2017-08-31 | 2017-12-22 | 山东精工电子科技有限公司 | The preparation method of high performance spherical nickel cobalt lithium aluminate cathode material |
| CN108232185A (en) * | 2017-12-18 | 2018-06-29 | 佛山市德方纳米科技有限公司 | The synthetic method of liquid phase doping ternary precursor |
| CN109336193A (en) * | 2018-10-21 | 2019-02-15 | 圣戈莱（北京）科技有限公司 | Multielement original position codope ternary material precursor and its preparation method and application |
| CN109896552A (en) * | 2019-02-19 | 2019-06-18 | 湖南中伟新能源科技有限公司 | A kind of preparation method for mixing aluminium lithium ion anode material presoma |
| CN111533183A (en) * | 2020-05-09 | 2020-08-14 | 中伟新材料股份有限公司 | Molten metal coated ternary precursor and preparation method thereof |
| CN114843504A (en) * | 2022-06-08 | 2022-08-02 | 中南大学 | Single-crystal-morphology lithium ion battery ternary positive electrode material and preparation method and application thereof |
| CN116969521A (en) * | 2023-07-31 | 2023-10-31 | 中国科学院过程工程研究所 | Sodium ion battery anode material precursor and preparation method and application thereof |
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| CN107500366A (en) * | 2017-08-31 | 2017-12-22 | 山东精工电子科技有限公司 | The preparation method of high performance spherical nickel cobalt lithium aluminate cathode material |
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| CN114843504A (en) * | 2022-06-08 | 2022-08-02 | 中南大学 | Single-crystal-morphology lithium ion battery ternary positive electrode material and preparation method and application thereof |
| CN116969521A (en) * | 2023-07-31 | 2023-10-31 | 中国科学院过程工程研究所 | Sodium ion battery anode material precursor and preparation method and application thereof |
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Application publication date: 20170510 |